Phenylacetone (P2P) synthesis from benzaldehyde with butanone

[MadHatter]

I guess what I'm really wondering about is the stochiometry of this reaction. In other write-ups of the bayer-williger I can't seem to find this enormous amounts of GAA. Can somebody help me with the rationale? I'm really close to trying this one out, but the amount of GAA is problematic.

 

[billythekid]

this amount of gaa is a lot and my best guess as to why is that preparing Peracetic acid in situ (during the reaction) and without a catalyst is inefficient so the chemist overcompensates to help with this, also GAA is used here as the solvent
by making the peracetic acid days before and testing the available oxygen content you are likely to get better results. This being said, I have seen professionals use this method and only get at best 35 to 65% of finished product. so an inexperienced chemist is likely to get even worse and a newbee is likely to fail or even worse hurt themselves. I recommend reading and studying and start small
make sure you thoroughly clean your finished reaction mix at the end of each step, Do not exceed -5c in the aldol condensation let mek/benzaldehyde stir overnight in the fridge after gassing.
do not exceed 60c in the Bayer villager. and research other oxidizers because I get better results with a different one.

 

[TheNut22]

My first try to do performic acid oxidation of MPB, to do it now better.
My MPB doesn't really mix to formic acid, as I put it in formic acid solution, buffered it with sodium carbonate, so
do I need a solvent for my MPB? If I do, can I use ethanol, or is acetone better? OrgUnikum? Someone? MadHatter?
I'll be VERY thankful because I don't want to mess up my reaction now, and I can give some tips for the procedure if it goes, and works well. AND, I don't have DCM... I haven't put it yet in the performic acid.

 

[TheNut22]

Or, can I use glacial acetic acid as the solution for my MPB also with my performic acid?

 

[Grubby]

Ya!ψ(｀∇´)ψThe RM after the reaction of benzaldehyde + MEK + HCI turns black and challenges the distillation of 3-Methyl-4-phenyl-3-buten-2-one with a boiling point of 269! This is the first time I bought a -60kpa vacuum pump for vacuum decompression and successfully obtained the golden yellow liquid 3-Methyl-4-phenyl-3-buten-2-one! But the machine seems to be overheated. Now I can only pause the distillation... Do you want the remaining rm to be completely distilled, right? I don’t want to distill out impurities with higher boiling points and ruin my hard work⋯

 

[Labchef]

Pls show your vacuum pump and how you used it in distillation please.

 

[Osmosis Vanderwaal]

That's some seriously red stuff. Usually the red to me is an abundance of hcl, but maybe not in this case, idk. I've found that 4:1, hcl(l) :H²SO⁴ is the equimolor amount, that uses up all of the sulfuric. Certainly 3:1 will still be gassing. Didnyou have a drying tube online with your gas?

 

[handle]

no drying tube on first attempt. will add the HCl acid directly to it next time.

 

[Osmosis Vanderwaal]

You could be right.mwhen I was look ing for my method, I discounted it because distilling the benzl alcohol out of paint thinner was the most viable method of obtaining Benz. Alc ( the chemical companies sell it but theynprerequisite want to know too much about what you are doing with something) but I noticed recently its on Amazon, so I can just click buy and there are no questions

 

[handle]

Yeah, its strange how countries regulate chemicals.. 1 different 1 from each country.

 

[Osmosis Vanderwaal]

It's not controlled, but filling out the Sima Eldredge work sheet is daunting. WHAT college or professional licensed business are you representing what the business tax ID? What do you plan to use it for? No thanks

 

[handle]

26th October 2024.
One method says to Chill and Ice MPB
Another method says to Heat and Reflux MPB
I just do both ?

 

[Labchef]

So you heat & reflux the MPB solution then chill in ice, do you get crystals when you do and are the crystals dry at room temperature.

 

[TheNut22]

I don't like to gas anything, because in my area concentrated sulfuric acid is banned. I was so relieved when I got very good results to just measure the ingredients, put the whole shebang together, start heating and watch a movie.

 

[TheNut22]

Performic acid procedure was like watching a horror movie with nasty panic attack. When I left to smoke a cigarette (4-5 min) and got back inside the flask was so hot it looked like it was boiling a little! Aaannnd, again VERY quickly under ice cool water ... After the long mixing process (~3,5 h) and having to do it with my hands (sweating and shaking), because 1 L flask doesn't fit to my heating mantle, I left it in cool water. I was shocked to read that it can explode in room temp with benzaldehyde! It is possible that there IS some, even when purified, but not distilled product. Well, I'm glad that the mixture is now in space where the temperature is under 20 C...

 

[handle]

that's what the fire diamond is for.
3 = Liquids that can be ignited under almost all ambient temperature conditions

 

[TheNut22]

Well, I succeeded, and good! And it's good to learn something new about chemistry, thanks, and, let's just say: Have a blast...
How I can stuff my dick into a condenser and the same time do vacuum "distillation"..

 

[B APPLE]

Teacher! Can you teach me how to synthesize methamphetamine from phenylacetone? Thank you

 

[B APPLE]

Excuse me! I poured methylphenylbutenone with acetic acid and 50% hydrogen peroxide Is it normal for the temperature to rise to 8-90 degrees on its own？

 

[Labchef]

What’s the color of your mixed MPB + acetic+ peroxide solution? I used commercial available peracetic acid. Solution color is dark brown but no rise temperature until heat was applied

 

[B APPLE]

I have now completed the production of phenoxyphenylpropene!

 

[B APPLE]

I saw that the teacher taught me to extract with chloroform. When I poured 800ml of chloroform down without layering, I was completely dumbfounded and spent a lot of material costs And the more I thought about it, the more unwilling I was to accept that after pouring chloroform and replacing it with DCM, the layers actually separated before using vacuum distillation to obtain it！

 

[B APPLE]

Let me tell you something interesting! I bought Diethyl Phenylacetate CAS20320-59-6 and easily obtained Phenylacetone. I obtained approximately 650ml of Phenylacetone from 1000ml of Diethyl Phenylacetate! Then I watched a video on the forum and wanted to purify phenylacetone! I mixed potassium carbonate with distilled water and phenylacetone, and the whole thing kept boiling! I want to say it's too bad to be reimbursed, but after boiling over 650, there's still 180 left But it's because of this that I know it's very pure! I don't understand chemistry very well, so sometimes I ask some basic questions but nobody pays attention! They have been using materials and testing themselves all along!

 

[B APPLE]

We are synthesizing more phenylacetone! I tried to synthesize methamphetamine from sodium borohydride but failed! The reason may be that the percentage of methylamine water is not high

 

[Labchef]

Can you share how you synthesize phenylacetone using diethyl phenylacetate. Is diethyl phenylacetate commercially available?